CN111187660A - 一种从磷虾中提取高品质磷虾油的方法 - Google Patents
一种从磷虾中提取高品质磷虾油的方法 Download PDFInfo
- Publication number
- CN111187660A CN111187660A CN202010033221.4A CN202010033221A CN111187660A CN 111187660 A CN111187660 A CN 111187660A CN 202010033221 A CN202010033221 A CN 202010033221A CN 111187660 A CN111187660 A CN 111187660A
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- Prior art keywords
- oil
- krill
- extraction
- krill oil
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 51
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- 239000002253 acid Substances 0.000 claims abstract description 22
- 235000021588 free fatty acids Nutrition 0.000 claims abstract description 14
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 91
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 70
- 238000000605 extraction Methods 0.000 claims description 65
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 32
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 23
- 238000004821 distillation Methods 0.000 claims description 15
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
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- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B1/102—Production of fats or fatty oils from raw materials by extracting in counter-current; utilisation of an equipment wherein the material is conveyed by a screw
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
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- C11B3/06—Refining fats or fatty oils by chemical reaction with bases
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Food Science & Technology (AREA)
- Microbiology (AREA)
- Nutrition Science (AREA)
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- General Chemical & Material Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Epidemiology (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Meat, Egg Or Seafood Products (AREA)
- Edible Oils And Fats (AREA)
- Fats And Perfumes (AREA)
Abstract
本申请公开了一种从磷虾中提取高品质磷虾油的方法。所述方法包括如下步骤:S1、将磷虾用有机溶剂进行提取,收集提取液;S2、向所述提取液中加入碱水,使游离脂肪酸形成脂肪酸盐从油相中分离出来、同时使油水分相,收集油相;S3、将所述油相进行纯化获得所述高品质磷虾油。本申请对磷虾油的制备工艺进行了优化,将有机溶剂萃取与碱炼法巧妙的结合,再通过对工艺参数进行调整、优化后,不仅降低了磷虾油的酸价,还最大程度的保证了磷虾油中磷脂、虾青素等有效成分的含量,提高了磷虾油的品质。
Description
技术领域
本发明涉及磷虾油制备领域,尤其涉及一种从磷虾中提取高品质磷虾油的方法。
背景技术
南极磷虾属于甲壳动物,全球海洋中约有85种磷虾,大约有7种到8种磷虾分布在南纬50度以南的环南极海域而被命名为南极磷虾。南极磷虾体长为5.5-6.0cm,寿命为5-7年,重量为2g左右,躯干呈透明状,繁殖能力强。在南极海域中,南极磷虾的生物量约为3.42-5.36亿吨,是全球单一物种蕴藏量最大的生物资源。南极磷虾营养丰富,包括蛋白质、脂类、抗氧化性物质,如虾青素、类黄酮及维生素A、E等。
南极磷虾油中脂类成分主要包括磷脂、甘油酯、游离脂肪酸和固醇等,其中磷脂含量丰富,与人体细胞中磷脂非常接近,易于被人体所吸收利用。南极磷虾油中ω-3多不饱和脂肪酸以磷脂形式存在,可以预防心脑血管疾病、炎性反应疾病、癌症、老年痴呆症、糖尿病、视力减退等6大疾病,且其活性优于目前市场上的甘油三酯型EPA/DHA产品及陆生植物来源的卵磷脂产品(其脂肪酸组成中不含EPA和DHA),是一种极具开发潜力的新型海洋生物功能成分。
游离脂肪酸(FFA)是影响南极磷虾虾油品质的重要因素之一,油脂中的游离脂肪酸,特别是多不饱和脂肪酸很容易被氧化生成过氧化物,过氧化物再分解为醛、酮等低分子量的挥发性成分,不仅会产生臭味,而且影响虾油的食用安全。因此,脱除南极磷虾虾油中的游离脂肪酸是高品质虾油生产的关键工艺之一。专利申请CN103602517A中公开了一种从磷虾中提取低酸价、低蛋白、低盐分含量磷虾油的方法,其得到的磷虾油的酸价(AV)在4.9-11.4mgKOH/g,该酸价仍不利于磷虾油的长期保存,长时间保存会影响磷虾油的粘度和透明度。因磷虾油中富含不饱和脂肪酸,与鱼油类似,根据鱼油标准SC/T 3502-2016,精制一级鱼油酸价≤1mgKOH/g,精制二级鱼油酸价≤3mgKOH/g,用正常原料制得的新鲜纯洁油脂,酸价很低,不超过2~3mgKOH/g,食用油脂的酸价不得高于3mgKOH/g。
脱除油脂中游离脂肪酸的方法有很多,如碱炼法、蒸馏法、溶剂萃取法、酯化法以及生物脱酸、超临界脱酸等,工业生产当中应用最广泛的是碱炼法;但是,碱性物质会造成局部中性油和极性磷脂发生皂化,同时游离脂肪酸皂化形成的皂脚极易吸附磷脂,从而造成有效成分的损失。
发明内容
针对现有技术中存在的缺陷,本发明的目的在于提供一种从磷虾中提取高品质磷虾油的方法,该方法对磷虾油的制备工艺进行了优化,将有机溶剂萃取与碱炼法巧妙的结合,对工艺参数进行了调整、优化,不仅降低了磷虾油的酸价,还最大程度的保证了磷虾油中磷脂、虾青素等有效成分的含量,提高了磷虾油的品质。
为达到以上目的,本发明采取的技术方案是:
本发明提供一种从磷虾中提取高品质磷虾油的方法,包括如下步骤:
S1、将磷虾用有机溶剂进行提取,收集提取液;所述提取液中溶剂为所述有机溶剂,溶质为磷虾油;所述磷虾可以为虾粉或块状磷虾或整个磷虾;
S2、向所述提取液中加入碱水,使游离脂肪酸形成脂肪酸盐从油相中分离出来(如充分搅拌方式)、同时使油水分相(如静置分层方式),收集油相;
S3、将所述油相进行纯化获得所述高品质磷虾油。
所述高品质磷虾油依磷虾原料的品质不同而不同,在相同条件下,该方法具有低酸价、高磷脂、高虾青素的优点。
一种优选的实施方式为,步骤S1中,所述有机溶剂为乙醇、丙酮、正己烷、乙醚、氯仿、乙酸乙酯中的任一种或任两种以上的混合物;优选乙醇;
所述有机溶剂的浓度为80~100%,优选90~100%,更优选95~100%。
一种优选的实施方式为,步骤S1中,所述提取时,所述磷虾与所述有机溶剂的料液比为1:(2~10),优选1:(3~9),更优选1:(3-6);
所述提取的方式为浸泡提取或逆流提取,优选逆流提取;
所述提取的温度为15-35℃,优选17-30℃,更优选19-22℃;
所述提取的次数为1~5次,优选2~3次;
每次所述提取的时间为0.3~2h,优选0.5~7h。
一种优选的实施方式为,步骤S2中,向所述提取液中加入碱水前,还包括将所述提取液进行浓缩的步骤,
优选的,所述浓缩的方式为第一减压蒸馏,
更优选的,所述第一减压蒸馏的温度为50~65℃,更优选60℃,
更优选的,所述第一减压蒸馏的真空度为-0.07Mpa~-0.1Mpa,
优选的,所述浓缩后的所述提取液中固形物的浓度为10~20%,更优选15%。
一种优选的实施方式为,步骤S2中,所述碱水的加入质量以水计为所述提取液质量的0.5~0.9倍,优选0.6~0.8倍,更优选0.7倍。
一种优选的实施方式为,步骤S2中,所述碱水中的溶质为碱性化合物,所述碱性化合物包括碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾、氢氧化钠、氢氧化钾、和氢氧化钙中的至少一种;优选碳酸钠或氢氧化钠;
所述碱性化合物为氢氧化钠,所述氢氧化钠的实际添加量为所述氢氧化钠的理论添加量的0.7~1.3倍,优选0.9~1.2倍,更优选1~1.1倍;所述氢氧化钠的理论添加量为M油×AV×7.14×10-4;所述M油为所述提取液中磷虾油的质量,所述AV为所述提取液中磷虾油的酸价;
所述碱性化合物为碳酸钠,所述碳酸钠的实际添加量为所述氢氧化钠的理论添加量的0.3~1.7倍,优选0.5~1.5倍,更优选1.5倍。
一种优选的实施方式为,步骤S2中,反应的温度为25~65℃,优选40~60℃,更优选45~55℃,更优选50℃。
一种优选的实施方式为,步骤S3中,所述纯化包括将所述油相溶于无水乙醇中,再经过滤和脱溶的步骤;
优选的,所述脱溶的方法为第二减压蒸馏;更优选的,第二减压蒸馏的温度和真空度与所述第一减压蒸馏的相同。
本发明还提供了一种高品质磷虾油,由以上任一所述方法制备得到,所述高品质磷虾油的剂型为胶囊剂、微囊剂、片剂、粉剂或水乳剂。
本发明还保护以上任一所述方法或所述高品质磷虾油在制备食品或药物中的应用,所述食品包括普通食品、保健食品、膳食补充剂、和特殊医学食品。
本发明的有益效果如下:
本发明通过向磷虾油提取液中加入碱水的方式,在去除磷虾油中游离脂肪酸降低酸价的同时,最大程度地保证了磷虾油中有效成分—磷脂的含量和虾青素的含量,得到的磷虾油具备高品质磷虾油的特点,可明显提升贮藏稳定性。另外,本发明方法还具有制备工艺操作简单,不需要添加额外增加脱酸设备的优点。本发明对工业化生产高品质磷虾油及其相关产品具有重要意义。
具体实施方式
下述实施例中所使用的实验方法如无特殊说明,均为常规方法。
下述实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。
下述实施例中:
得率(提油率)=所得虾油质量/所用虾粉质量×100%;
酸价定义为中和1g油脂中的游离脂肪酸,需要KOH或NaOH的毫克数。
实施例1、不加碱时磷虾油提取工艺及优化
从南极磷虾粉中制备磷虾油的方法,包括如下步骤:
S1、南极磷虾粉经有机溶剂(乙醇)逆流提取,得提取液;
S2、将步骤S1所得提取液减压蒸馏,得到浓缩液;
S3、在步骤S2的浓缩液中加入纯化水精制,充分混匀后静置至分层,收集下层粗油;
S4、将步骤S3的下层粗油与无水乙醇混合后静置,过滤,保留溶解液;
S5、步骤S4的溶解液加热减压蒸馏脱溶,得到纯化精制磷虾油。
步骤S1中,磷虾粉中水分含量和乙醇浓度高低会影响磷虾油的品质、提取率、有效物质的含量,磷虾粉中水分含量高,将稀释萃取溶剂乙醇的浓度,随着乙醇浓度的降低,提取率降低,磷脂含量提高,但虾青素、透明度降低,粘度增高,当乙醇浓度低于90%后,磷虾油品质差,乙醇浓度优选90%、95%、100%。
步骤S2中,所述减压蒸馏,温度范围50℃-65℃,优选60℃,所述减压真空度范围-0.07Mpa~-0.1Mpa;所述浓缩液中固形物的浓度为10%-20%,优选15%。
步骤S3,所述纯化水添加比例为浓缩液质量的50%-90%,加水物理沉降过程中水的用量会影响提取率及磷虾油的品质,在此用量范围内,提油率较高,所得磷虾油中磷脂含量较高,为同时保证磷脂含量和提油率加水量优选70%;静置时间为1h-8h,优选4h;加入纯化水的精制过程是根据磷脂的亲水性,在此过程中不具有亲水活性的或已经变性的磷脂不会吸水沉降,并可去除一部分杂质、游离脂肪酸、蛋白质、多糖、盐分等,所获得的磷虾油粗油中的磷脂DHA、EPA等不饱和脂肪酸及虾青素等有效成分明显提高,而且所获得的磷虾油的品质(流动性和透明度)明显提高。
步骤S4,所述无水乙醇的用量为下层粗油质量的1-5倍。在此用量范围内,提油率较高,所得磷虾油中磷脂含量较高,生产成本最低。无水乙醇最优选的为下层粗油质量的3倍。
步骤S5,所述减压蒸馏工艺参数同步骤S2;所述纯化精制的磷虾油中含有具有活性的磷脂(包括2%-20%醚磷脂和25%-55%非醚磷脂)、胆碱(≥5%)、甘油三酯、Omega-3不饱和脂肪酸及Omega-6不饱和脂肪酸等多不饱和脂肪酸、饱和脂肪酸、游离脂肪酸等。精制纯化后的磷虾油纯净、透明,磷脂、虾青素、Omega-3不饱和脂肪酸含量高,可应用于普通食品、保健食品、膳食补充剂、功能食品、特殊医学食品中,剂型可为胶囊剂、微囊剂、膏剂、片剂、粉剂或水乳剂等。
一、不同料液比和提取温度的提取效果比较
以南极磷虾粉为原料,按照上述步骤S1-S5制备磷虾油,其中,有机溶剂为95%乙醇溶液,提取时间为40-41min,浓缩液中固形物的浓度为15%,步骤S3中加水量为浓缩液质量的70%,静置时间为4h,所述减压蒸馏的温度为60℃,真空度范围-0.07Mpa~-0.1Mpa,设置不同料液比(磷虾粉与有机溶剂的质量比)和不同的提取温度,比较最后获得的磷虾油的提取效果,如表1所示。
表1中编号1-1、1-4、1-5和1-6的结果比较可以得出,提油率随着料液比的增大而升高,磷虾油中磷脂含量随着料液比的增大而降低,磷虾油中虾青素含量随着料液比的增大而升高;料液比1:6与1:9提油率差异不大,说明料液比1:6时,磷虾粉中脂肪绝大部分已经提取出来,料液比增加到1:9,生产成本、乙醇回收压力大幅升高,综合考虑磷脂、虾青素、提取率及生产成本,采取1:6的料液比;编号1-1、1-2、1-3的结果比较可以得出,提取温度为20℃时提油率、磷脂含量和虾青素含量相对较高且稳定高,综合来看,提取温度为20℃整体效果较好。
表1、不同料液比和提取温度的效果比较
二、不同有机溶剂浓度及不同原料含水量的提取效果比较
1、以南极磷虾粉为原料,按照步骤一的方法进行提取,不同之处在于:料液比为1:3,提取次数为2次,每次提取1h,提取温度为室温(20-30℃),步骤S3获得的粗油直接脱溶蒸干,有机溶剂为不同浓度的乙醇溶液,比较最终获得的磷虾油提取效果如表2所示。
2、以不同含水量的南极磷虾粉为原料,按照步骤1的方法进行提取,不同之处在于:有机溶剂为无水乙醇,比较最终获得的磷虾油提取效果如表3所示。
表2结果显示,有机溶剂中乙醇浓度越高,提油率越高,磷虾油中磷脂含量越低,虾青素含量越高,另外,表2结果与表1结果相比,提油率明显提高,料液比低于表1,但磷脂含量和虾青素含量却低于表1结果,说明将步骤S3获得的粗油直接脱溶蒸干,粗油中大量杂质未去除,明显降低磷脂含量和虾青素含量。表3结果显示,原料中含水量越高,提油率越低,磷虾油中磷脂含量越高,虾青素越低。即磷虾粉中水分含量和乙醇浓度高低会影响磷虾油的品质、提油率、有效物质的含量,随着乙醇浓度的降低,提取率降低,磷脂含量提高,但虾青素、透明度降低,粘度增高,当乙醇浓度低于90%后,磷虾油品质差,乙醇浓度优选90%、95%、100%。
表2、不同浓度溶媒的效果比较
表3、磷虾粉中水分含量对磷虾油提取的影响
三、不同有机溶剂浓度、浓缩液浓度、加水量的提取效果比较
以南极磷虾粉为原料,按照步骤一的方法进行提取,不同之处在于:料液比为1:3,提取次数为3次,每次提取0.5h,提取温度为室温(20-30℃),有机溶剂为不同浓度的乙醇溶液,浓缩液浓度为10-15%,加水量为浓缩液质量的50%-70%,比较提取效果如表4所示。
表4中编号3-2、3-4、3-5结果显示,乙醇浓度越高,提油率越高,磷虾油中磷脂含量越低,虾青素含量越高;编号3-1和3-2的结果显示,加水量为70%时的提油率、磷脂含量、虾青素含量均较高;编号3-1和3-3的结果显示,浓缩液浓度为15%时的提油率和磷脂含量均较高,虾青素含量较低。综合提油率、磷脂及虾青素含量,优选浓缩液浓度为15%,加水量为70%。具体可根据生产实际,调整有机溶剂浓度90%-100%、浓缩液浓度10-15%、加水量比例50-70%,得到磷脂含量40%-75%的南极磷虾油。
表4、不同有机溶剂浓度、浓缩液浓度、加水量的效果比较
实施例2、加碱脱酸及工艺优化
以南极磷虾粉为原料,按照实施例1的方法进行提取,不同之处在于:将水替换为碱水,将南极磷虾提取液浓缩至固形物含量为10%~20%,加入浓缩液质量0.5~0.9倍的碱水(以水计),搅拌1小时,搅拌温度为25℃~60℃,搅拌速率为400-1000rpm/min;搅拌后静置至分层,取下层油相,溶于无水乙醇中,过滤;滤液真空脱溶,获得精制南极磷虾油。
所述碱水的配制:碳酸钠(纯碱)或氢氧化钠(烧碱)溶于去离子水进行配制;烧碱实际添加量为0.9~1.2倍烧碱理论添加量,纯碱实际添加量为烧碱理论添加量的0.5~1.5倍。
所述烧碱理论添加量的计算公式为MNaOH=M油×AV×7.14×10-4,MNaOH为烧碱理论添加量(单位kg),M油为所述南极磷虾粗油的质量(单位kg),AV为所述南极磷虾粗油的酸价(单位mgKOH/g油)。
一、不同碱与用量及不同碱处理温度的效果比较
以南极磷虾粉为原料,按照实施例1中编号为3-2方法得到提取液,浓缩至浓缩液中固形物含量为15%,按照前述方法加入不同量和不同种类的碱水,搅拌1小时,搅拌温度为25~60℃,搅拌速率为400-1000rpm/min;搅拌后静置至分层,取下层油相,溶于无水乙醇中,过滤;滤液真空脱溶,获得精制南极磷虾油。结果如表5所示。
表5中4-3、4-4、4-5、4-6的结果显示,碱水中使用烧碱时,烧碱的实际添加量为烧碱理论添加量的1.1倍时效果最佳(酸价相对较低,得率、磷脂含量、虾青素含量变化不大),4-7、4-8、4-9的结果显示,使用碱水时反应温度在50℃时效果最佳,即烧碱的实际添加量为理论添加量的1.1倍、使用碱水时反应温度在50℃时的方案最佳,结果如4-10所示。
表5中编号4-11、4-12、4-13的结果显示,碱水中使用纯碱时,纯碱的实际添加量为烧碱理论添加量的1.5倍时效果最佳(酸价相对较低,得率、磷脂含量、虾青素含量变化不大),编号4-14、4-15、4-16的结果显示,使用碱水时反应温度在50℃时效果最佳,即纯碱的实际添加量为烧碱理论添加量的1.5倍、使用碱水时反应温度在50℃时的方案最佳,结果如编号4-15所示。
表5、不同碱用量及不同碱处理温度的效果比较
二、水/碱水处理后的粗油直接脱溶蒸干
以南极磷虾粉为原料,按照步骤一中编号4-10的方法进行提取,不同之处在于:料液比1:3,提取次数为3次,每次提取0.5h,提取温度为室温(20-30℃),有机溶剂为95%乙醇,浓缩液中固形物的浓度为15%,加水量为浓缩液质量的70%,经水/碱水处理后的粗油直接脱溶蒸干粗油,碱水的溶质使用氢氧化钠,实际添加量为1.1倍理论加碱量,最终获得的磷虾油结果如表6所示。
表6结果表明,与加入纯水相比,加入碱水后获得的磷虾油酸价明显降低,虾青素含量明显升高,但提油率和磷脂略有降低。
将表6结果与表5编号4-10的结果比较发现,粗油直接脱溶蒸干与将粗油通过无水乙醇溶解、过滤、减压脱溶后的酸价相同,说明将粗油通过无水乙醇溶解、过滤、减压脱溶的工艺不会对酸价产生影响,但可以提高磷虾油中虾青素含量,使磷脂含量略有降低。
表6、水/碱水处理后的粗油直接脱溶蒸干
综上,通过脱酸可有效减低磷虾油酸价,提高磷虾油贮藏稳定性。实施例2的加碱脱酸通过公式计算即可得到碱的添加量,并且不用额外增加脱酸设备,生产投入较低,脱酸效果明显,但碱水添加量(以水计)超过浓缩液质量的1倍,将降低磷虾油成品的透明度,且得率下降。
本说明书中未作详细描述的内容属于本领域专业技术人员公知的现有技术。以上所述仅为本申请的实施例而已,并不用于限制本申请。对于本领域技术人员来说,本申请可以有各种更改和变化。凡在本申请的精神和原理之内所作的任何修改、等同替换、改进等,均应包含在本申请的权利要求范围之内。
Claims (10)
1.一种从磷虾中提取高品质磷虾油的方法,其特征在于,包括如下步骤:
S1、将磷虾用有机溶剂进行提取,收集提取液;
S2、向所述提取液中加入碱水,使游离脂肪酸形成脂肪酸盐从油相中分离出来、同时使油水分相,收集油相;
S3、将所述油相进行纯化获得所述高品质磷虾油。
2.根据权利要求1所述的方法,其特征在于,步骤S1中,所述有机溶剂为乙醇、丙酮、正己烷、乙醚、氯仿、乙酸乙酯中的任一种或任两种以上的混合物;优选乙醇;
所述有机溶剂的浓度为80~100%,优选90~100%,更优选95~100%。
3.根据权利要求1或2所述的方法,其特征在于,步骤S1中,所述提取时,所述磷虾与所述有机溶剂的料液比为1:(2~10),优选1:(3~9),更优选1:(3-6);
所述提取的方式为浸泡提取或逆流提取,优选逆流提取;
所述提取的温度为15-35℃,优选17-30℃,更优选19-22℃;
所述提取的次数为1~5次,优选2~3次;
每次所述提取的时间为0.3~12h,优选0.5~7h。
4.根据权利要求1-3中任一所述的方法,其特征在于,步骤S2中,向所述提取液中加入碱水前,还包括将所述提取液进行浓缩的步骤,
优选的,所述浓缩的方式为第一减压蒸馏,
更优选的,所述第一减压蒸馏的温度为50~65℃,更优选60℃,
更优选的,所述第一减压蒸馏的真空度为-0.07Mpa~-0.1Mpa,
优选的,所述浓缩后的所述提取液中固形物的浓度为10~20%,更优选15%。
5.根据权利要求1-4中任一所述的方法,其特征在于,步骤S2中,所述碱水的加入质量以水计为所述提取液质量的0.5~0.9倍,优选0.6~0.8倍,更优选0.7倍。
6.根据权利要求1-5中任一所述的方法,其特征在于,步骤S2中,所述碱水中的溶质为碱性化合物,所述碱性化合物包括碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾、氢氧化钠、氢氧化钾、和氢氧化钙中的至少一种;优选碳酸钠或氢氧化钠;
所述碱性化合物为氢氧化钠,所述氢氧化钠的实际添加量为所述氢氧化钠的理论添加量的0.7~1.3倍,优选0.9~1.2倍,更优选1~1.1倍;所述氢氧化钠的理论添加量为M油×AV×7.14×10-4,所述M油为所述提取液中磷虾油的质量,所述AV为所述提取液中磷虾油的酸价;
所述碱性化合物为碳酸钠,所述碳酸钠的实际添加量为所述氢氧化钠的理论添加量的0.3~1.7倍,优选0.5~1.5倍,更优选1.5倍。
7.根据权利要求1-6中任一所述的方法,其特征在于,步骤S2中,反应的温度为25~65℃,优选40~60℃,更优选45~55℃,更优选50℃。
8.根据权利要求1-7中任一所述的方法,其特征在于,步骤S3中,所述纯化包括将所述油相溶于无水乙醇中,再经过滤和脱溶的步骤;
优选的,所述脱溶的方法为第二减压蒸馏;更优选的,第二减压蒸馏的温度和真空度与所述第一减压蒸馏的相同。
9.一种高品质磷虾油,由权利要求1-8中任一所述方法制备得到,所述高品质磷虾油的剂型为胶囊剂、微囊剂、片剂、膏剂、粉剂或水乳剂。
10.权利要求1-9中任一所述方法或所述高品质磷虾油在制备食品或药物中的应用,所述食品包括普通食品、保健食品、膳食补充剂、和特殊医学食品。
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